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Environmental Monitoring at W-Block, Greater Kailash-II, New Delhi

INTRODUCTIONThe Environmental Monitoring was carried out by the environment team of Spectro Analytical Labs Ltd. at DLF Residential Complex at W-Block, Greater Kailash- II, New Delhi. Being a construction and development company DLF is very much concerned about to reduce the environmental impact due to its Constructional and Operational activities. The present work is concerning the existing environmental condition with respect to water, waste water, air and noise levels.

Environmental monitoring programme is a vital process of any management plan of the operational & development. This helps in signaling the potential problems that result in from the project and will allow for prompt implementation of effective corrective measures. The environmental monitoring will be required for both the construction and operational phases. The main objectives of environmental monitoring are:

Assess the changes in environmental conditions;

Monitor the effective implementation of mitigation measures;

Warn significant deteriorations in environmental quality for further prevention action.

In order to meet the above objectives the following parameters need to be monitored:

Water Quality;

Ambient Air and Noise quality

Scope of work and the detail of the sampling are given in the following paragraphs:-

Spectro Analytical Labs Ltd. 1 of 41


SCOPE OF WORKThe scope for performing the environmental monitoring is already mentioned in the work order, which is briefly given

for ready reference.

1. Monitoring of Ambient air quality for the parameters namely PM 10, PM 2.5, Sulphur dioxide (“SO2”) & Oxides of Nitrogen (“NO2”), Carbon Monoxide (“CO”), Ozone (“O3”), Lead (“Pb”), Ammonia (“NH3”), Benzene (“C6H6”), Benzopyrene (“BaP”), Arsenic (“As”), and Nickel (“Ni”), at the project site Monitoring of Ambient Noise Level Monitoring (24-hrs, day & night Leq) at two locations (one at the project site & other within the boundary of the project site).

2. Collection and Analysis of the Ground water samples from project site.

3. Collection and Analysis of Soil Sample from project site.

4. Monitoring of Ambient Noise Level (24 hrs) at the project site and at the project boundary



Abbreviations used in the Report

PM 10 = Particulate Matter (< 10 micron sized particle)

PM 2.5 = Particulate Matter (< 2.5 micron sized particle)

GL = Ground Level;

SO2 = Sulfur Dioxide

NO2 = Nitrogen Dioxide

AAQ = Ambient Air Quality

dB = decibel

N.D = Not detected

MDL = Minimum Detection Limit



INSTRUMENTS & APPARATUS

Air (Particulate Matter, PM 10) Monitoring Instrument

Instrument Make Model No. InstrumentIdentification

No.

Range and Sensitivity

SPM/RSPM GasesRespirable

Dust Sampler (RDS)

M/s. Spectro Instruments Pvt. Ltd. – New Delhi

SLE -RDS 103/SLE -GA 133

SAL/RDS/10, 13 0.02 – 01.8 m3/min

±0.02 m3/min

0.2 – 3 LPM

± 0.2 LPM

Filter Paper Details

APPRATUS MAKE SIZE SIZE PRODUCTCATEGORY NO.

Filter Paper M/S Whatmann International Ltd.

20.3 x 25.4cm GF/ACAT NO. 1820-866

Air (Particulate Matter, PM 2.5) Monitoring Instrument

Instrument Make Model No. InstrumentIdentification

No.

Range and Sensitivity

PMFine

Particulate Sampler

M/s. Spectro Lab

Equipments Pvt. Ltd.

SLE-FPS 105

SAL/FPS/01&2 16.67 LPM

Filter Paper Details

APPRATUS MAKE SIZE SIZE PRODUCTCATEGORY NO.

Filter Paper M/S Whatmann International Ltd.

47 mm GF/A & EPM 2000

Noise (Sound) Measuring Instrument



Instrument Make Model No. Instrument Identification

Detection Limit

Integrated Sound Level Measurement Instrument Standard Accessories

Baseline Technologies

2001

A0907-980

SAL/NOISE/INT/692

Lo 30-100dB

Hi 60-130dB



Testing Methods Followed


S.No. Particular Testing Method to be Followed

1 Ambient Air Monitoring ParameterA PM 10 IS-5182 (part – 23) 1973, Handbook of Methods in

Environment Studies (Vol 2) Published by ABD

Publication – Jaipur

B PM 2.5

C SO2 (Sulfur Dioxide) IS 5182 (Part – II) 1969, with Improved West &

Gaeke MethodD NO2 (Nitrogen Dioxide) Modified Jacobs – Hochheiser Method / Arsenite

Method

E Carbon Monoxide (as CO),

(mg/m3)

Gas Chromatography

F Ozone (as O3) (µg/m3) Chemical Method

GLead (as Pb) (µg/m3)

AAS Method after sampling on EPM 2000 or

equivalent filter paper

H Ammonia (as NH3)

(µg/m3)

Chemiluminescence

I Benzene (as C6H6)

(µg/m3)

Gas chromatography based continuous analyzer

J Benzo (O) Pyrene (as BaP)

(ng/m3)

Solvent extraction followed by HPLC/GC analysis

K Arsenic (as As) (ng/m3) AAS Method after sampling on EPM 2000 or

equivalent filter paperL Nickel (as Ni) (ng/m3)

2 Noise Level MeasurementA Noise Level in dB (A) for

continuous 24 hours

Operational Manual of Noise level Meter, Model

No. SL 5868 issued by Baseline Technologies

3 Water Analysis

Standard Method for the Examination of Water & Wastewater, 21st Edition, Edited by Lenore S.

Clesceri, Arnold E. Greenberg, Andrew D. Eton is followed for analysis.

4 Soil Analysis: As per Protocol: FAO / IS: 2720


RESULTS OF AMBIENT AIR QUALITY




ID: 1110050079

Ambient Air Analysis Report

Name of the Project - Residential Complex W-Block, Greater Kailash-II, New Delhi.

Name & Address of the Company - M/s DLF LTD, DLF Centre, Sansad Marg, New DelhiName of the Site - Residential Complex, W-Block, Greater Kailash-II, New

DelhiLocation of Sampling Point - At the Project SiteDate of Sampling - 20/10/2011Sampling Started at - 11.00 A.M. (20.10.11)Sampling Completed at - 11.00 A.M. (21.10.11)Actual Time of Sampling (minutes) - 1440Av. Flow Rate for SPM (m3/min.) - 1.11 Total Volume of Air Sampled for SPM (m3)

- 1584Average Ambient Temperature (oC)

- 25Purpose of Monitoring - To Assess Pollution Load

PARAMETERS RESULTS Limits as per CPCB (MOEF)

Industrial,Residential, Rural

& other areas

Ecologically SensitiveArea (notified by

Central Government)

Particulate Matter PM 2.5 (µg/m3) - 87 60 60Particulate Matter PM 10 (µg/m3) - 140 100 100Sulphur Dioxide (as SO2) (µg/m3) - < 5.0 80 80Oxides of Nitrogen (as NO2) (µg/m3) - 23.5 80 80Carbon Monoxide (as CO), (mg/m3) - 1.1 02 02Ozone (as O3) (µg/m3) - 21.2 100 100Lead (as Pb) (µg/m3) - N.D 1.0 1.0Ammonia (as NH3) (µg/m3) - 11.3 400 400Benzene (as C6H6) (µg/m3) - N.D 05 05Benzo (O) Pyrene (as BaP) (ng/m3) - N.D 01 01Arsenic (as As) (ng/m3) - N.D 06 06Nickel (as Ni) (ng/m3) - N.D 20 20

Protocol – IS: 5182 (Pt - 4, 6 & 23) / IS: 2488, IS-13270


RESULTS OF SOIL ANALYSIS



ID: 1110050079

Soil Analysis Report

S.No TESTS RESULTS

1 pH value 7.32

2 Conductivity, milliohms/cm 0.23

3 Bulk Density (g/cc) 1.42

4 Total Nitrogen (as N), % w/w 0.06

5 Total Organic Matter, % w/w 0.055

6 Phosphates (as P), mg/kg 4.89

7 Sodium (as Na), mg/kg 39.77

8 Potassium (as K), mg/kg 9.94

9 Calcium (as Ca), mg/kg 810.38

10 Magnesium (as Mg), mg/kg 47.23

11 Water holding capacity, % w/w 44

12

Texture

a. Sand, % w/w

b. Silt, % w/w

c. Clay, % w/w

62.58

26.69

10.73

Protocol: FAQ / IS: 2720



RESULTS OF NOISE MONITORING



ID: 1110050079Date: 20/10/11 to 21/10/11

AMBIENT NOISE MONITORING REPORT (W-Block, Greater Kailash)Location: Near Entry Gate


Time Hourly LeqdB (A)

Result dB (A)

MIDNIGHT 53.6 Leq 69.21:00 AM 53.2 L10 73.5

2 52.0 L50 71.93 52.4 L90 69.84 51.3 Lday 70.85 53.1 Lnight 58.86 56.5 Ldn 70.37 62.0 Lmax 73.88 67.0 Lmin 51.3

9 70.2

10 72.7

11 73.6

12 NOON 71.6

13 73.0

14 72.1

15 70.5

16 70.4

17 73.8

18 72.2

19 71.6

20 68.3

21 65.4

22 60.4

23 58.1

Area Category of Area Limits in day (dB)

Limits in Night (dB)

A Industrial 75 70B Commercial 65 55C Residential 55 45D Silence Zone 50 40


RESULTS OF WATER SAMPLE



ID: 1110050079RESULTS OF RAW WATER

TESTS RESULTS LIMITS (MAX) PROTOCOLSDesirable Extended

Colour, Hazen Units

<5.0 5 25 IS- 3025(Pt-4): 1983

Odour Unobjectionable Unobjectionable IS- 3025(Pt-5): 1983

Taste Agreeable Agreeable IS- 3025(Pt-7&8): 1984

Turbidity, NTU <1.0 5 10 IS- 3025(Pt-10): 1984

pH Value 7.58 6.5 to 8.5 IS- 3025(Pt-11): 1984

Total Dissolved Solids, mg/l

786 500 2000 IS- 3025(Pt-16): 1984

T. Hardness (asCaCO3), mg/l

404 300 600 IS- 3025(Pt-21): 1983

Residual Free Chlorine, mg/l

0.2 0.2 (Min) When Chlorinate 45 of IS-3025: 1964

Chlorides (as Cl), mg/l

195.68 250 1000 IS-3025(Pt-32): 1984

Total Iron (as Fe), mg/l

0.16 0.3 1.0 32 of IS- 3025: 1964

Fluorides (as F), mg/l

0.37 1.0 1.5 APHA-4500-D-F

BACTERIOLOGICAL TESTS


TESTS RESULTS LIMITS PROTOCOLSTotal Coli-forms /100ml (MPN)

< 2.0 10 (Max) IS: 1622-2003

E. Coli/100ml Absent Absent IS: 1622-2003


MONITORING AND ANALYSIS METHODOLOGY

The IS methods are followed to decide the monitoring stations, analysis of different sample and also alternative

methods are used, where the cross verification is required.

[A] Ambient Air Quality Monitoring:

Two Respirable Dust Samplers (RDS) with gaseous attachment have been used for RSPM/SPM Sampling. RDS with

Gaseous attachment assembly is used for the collection of gaseous pollutants such as SO 2, NO2 and CO. The details of

the instrument used for sampling is mentioned in the separate annexure under the heading of details of Instruments &

Apparatus. For the measurement of fine particulate matter having an aerodynamic dia. Less than or equal to a nominal

2.5 micrometer (PM2.5). Draw ambient air at a constant flow rate of 16.67 Lpm .Total volume of the sampled air is

automatically computed by the sampler from the measured sampling flow rate .the mass concentration of PM 2.5

particles in the ambient air is computed by dividing the total mass of collected particles by the total volume of sample

air and is expressed in micro grams per cubic meter of air.37mm glass fiber filter and 1 ml of diffution oil or silicon oil.

For the collection of PM2.5 particulate matter we use 47mm PTFE (polytetrafluoro ethylene). The ambient air enter the

sampler air inlet and pass through the size selective inlet particles larger then 10micro are separated . it then moves

through down tube to the impacter where particles larger then 2.5 micro are cut off.the particles smaller then 2.5 micro

are then collected on a filter paper (47mm PTFE ) mounted in a filter cassette and kept in a holder .

[B] Water Quality Survey:

Water samples were collected in Pre-sterilized sampling container. Chemical and Bacteriological analysis was carried

out as per standard Methods for water and Wastewater Analysis, Published by IS, APHA, etc.

[C] Noise Level Measurement:

Instant sound level meter is used for the collection of data related to noise for continuous 24 hours and for D.G. Set. The

details of the instrument used for the sampling is mentioned in the separate annexure under the heading of Details of

instruments & Apparatus.



METHODOLOGY OF AMBIENT AIR QUALITY



PARTICULATE MATTER (PM 2.5)

Introduction

PM larger than 2.5 microns and less than 10 microns is mostly produced by mechanical processes. These include automobile tire wear, industrial processes such as cutting and grinding, and re-suspension of particles from the ground or road surfaces by wind and human activities.

PM less than or equal to PM2.5 is mostly derived from combustion sources, such as automobiles, trucks, and other vehicle exhaust, as well as from stationary combustion sources.

Methodology to Calculate PM 2.5

For the measurement of fine particulate matter having an aerodynamic dia. Less than or equal to a nominal 2.5 micrometer (PM2.5). Draw ambient air at a constant flow rate of 16.67 Lpm .Total volume of the sampled air is automatically computed by the sampler from the measured sampling flow rate .the mass concentration of PM 2.5 particles in the ambient air is computed by dividing the total mass of collected particles by the total volume of sample air and is expressed in micro grams per cubic meter of air .

37mm glass fiber filter and 1 ml of diffution oil or silicon oil.

For the collection of PM2.5 particulate matter we use 47mm PTFE (polytetrafluoro ethylene). The ambient air enter the sampler air inlet and pass through the size selective inlet particles larger then 10micro are separated . it then moves through down tube to the impacter where particles larger then 2.5 micro are cut off.the particles smaller then 2.5 micro are then collected on a filter paper (47mm PTFE ) mounted in a filter cassette and kept in a holder .

CALCULATION

The PM 2.5 concentration is calculated

PM 2.5= (Wf- Wi) / Va

Wf= Final Weight (gm)

Wi= Initial Weight (gm)

Va= Total Air Vol. sampled in actual Vol. units (m3)



RESPIRABLE PARTICULATE MATTER

Principle Ambient air laden with suspended particulates enters the system through the inlet pipe. As the air passes through the cyclone, coarse, non-Respirable dust is separated from the air stream by centrifugal forces acting on the solid particles. The separated particles fall through the cyclone’s conical hopper and collected in the sampling bottle placed at its bottom. The fine dust forming the repirable fraction of the total suspended particulate matter passes through the cyclone and is carried by the air stream to the filter paper clamped between the top filter cover and the filter adopter assembly. The respirable dust is retained by the filter and the carrier air exhausted from the system through the blower.

RESPIRABLE SIZE CUT OFFThe repirable dust standard recommended by the Central pollution Control Board is a 10 micron cut off size for respirable dust measurement. Moreover, the respirable tract like any other inspection centrifugal separation system retains particulates with varying densities at different levels. This implies that even relatively finer dust particles of materials having a higher specific gravit5y are likely to be retained in the upper respiratory tract while large particulates of lighter materials are likely to pass deeper into the respiratory system.

II) Procedure of sample collection:

Following steps are involved in the collection of samples;

a) Open the shelter of Respirable Dust Sampler (RDS), loosen the wing nuts and remove the retaining ring from the filter holder.

b) Mount a pre-weighted and numbered glass fibers filter paper in position with the rough side up and tighten the wing nuts.

c) Allow the RDS to run for the specified length of time (24 hrs)d) During the sampling time, flow rate should be taken hourlye) At the end of sampling remove the filter form the mount very carefully.f) Fold the filter in half upon itself with the collected materials enclosed within.g) Place the folder filter in a clean, tight envelope and mark it for identification.h) Place the filter in a desicator.

ANALYSIS OF SAMPLES:

In a lab. remove the filter from the desicator and take out the filter paper from the envelope. Examine the inside surface of filter paper and with the pair of tweezers; remove any accidental objects such as insects. Dry the filter paper by keeping on watch glass in hot air oven at 1050 C for about one hour. Equilibrate the exposed filters for about one hour in desicator. Carry the desicator to the balance and weight on the analytical balance to the nearest 0.1-milligram.

I) Calculation of volume of air sampled:

V =Q x T



Where

V= Air volume sampled (m3 )

Q = Average flow rate ( m3 per minute)

T = Sampling Time (in minutes)

( Q1 + Q2)Q = 2

Q1 = Initial sampling rate indicated by the orifice meter at the start of sampling

Q2 = Final sampling rate indicated by the orifice meter just before the end of sampling.

II) Calculations of mass concentration of Responded particulate Matter (RPM):

The mass concentration of RPM may be calculated as follows:

( Fw – Iw ) x 106

RPM (μg/m3) = ----------------------- VWhere

Fw = Final weight of exposed filter paper in grams.

Iw = Initial weight of unexposed filter paper in grams.

V = Air volume sampled in cubic meter.

Weight of dust retained by the cyclone SPM (μg/m3) = RPM (μg/m3) + ------------------------------------------------------ Volume of air sampled, m3



METHODS FOR DETERMINATION OF OXIDES OF NITROGEN IN AMBIENT AIR

PrincipleThe collection and fixation of nitrogen dioxide in air is done by scrubbing a known volume of air through a solution of basic sodium arsenate. The absorbed nitrogen dioxide is determined calorimetrically as the azo dye by using it to diazotize sulphanilamide in the presence of phosphoric acid at a pH of less than 2 and then coupling it with N-(1-Naphthyl)-ethylenediamine dihydrochloride. The method is standardized statically by using NaNO2 standard. Standardization is based upon the empirical observation that 0.74 mole of NaNO2 produces same colour as 1 mole of NO2. The absorbance of the highly colored azo dye is measured on a spectrophotometer at a wavelength of 540 nm.

Range and SensitivityAnalysis in the range of 0.04 to 2.0 μg/ml can be performed by this method. The monitoring range of the method is 9 to 750 μg/ml. However, under certain conditions, with a sampling rate of 2.0 LPM for 24 hours, a sampling efficiency of 82% the range of the method is 9 to 450 μg/m3. Nitrogen dioxide in the range of 420-750 μg/m3 is accurately measured by 1.1 dilution of the collected sample.

THE GASEOUS SAMPLING ATTACHMENTSA trapping is drawn from the suction side of the blower below the orifice plate assembly to provide suction for sampling air through a set of impingers. These impingers are housed in a separate enclosures and kept in an ice tray.

The separate enclosure and ice tray insulate the impingers from ambient temperature and heat generated in the motor of the blower. It has Gas Manifold and Rotameter to allow setting up of independent sampling rates through each of impingers.

The gaseous sampling attachment can easily be detached from the main sampler and transported and stored independently.

CALCULATIONI) The concentration of nitrogen dioxide in microgram per meter cube in the sample may be calculated as

follows:

NO2 (μg/m3 ) = (A-Ao) x F x Vf -------------------------- Va x Vt x 0.82Where

A= Sample Absorbance

Ao= Reagent blank absorbance



INTERFERENCESulphur dioxide is a major interference due to nitric oxide is positive while that due to carbon dioxide is negative. Interference from sulphur dioxide can be eliminated by converting it to sulphuric acid by the addition of hydrogen peroxide.



METHOD FOR DETERMINATION OF SULPHUR DIOXIDE IN AMBIENT AIR

Principle:

When sulphur dioxide from the air is absorbed in a sodium tetrachloromercurate solution it forms a stable sodium dichloro-sulphitomercurate solution. The amount of sulphur dioxide is then estimated by the colour produced when pararosaniline hydrochloride is added to the solution. The magenta colour is produced and estimated at 560 nm.

Range & SensitivityThe measurement should be reported to the nearest 0.005 ppm at concentration below 0.15 ppm and to the nearest 0.01 ppm above 0.15 ppm.

Interference Ozone and nitrogen dioxide interfere if presents in the air sample at concentration greater than sulphur dioxide. Interference of nitrogen dioxide is eliminated by adding 0.06 percent sulphamic acid in the absorbing reagent. Nitrogen dioxide interference may also be eliminated by adding 0.1 tuluidine after sample collection. Heavy metals interfere by oxidizing dichloro-sulphitomercurate during sampling collection. The interference is eliminated by adding EDTA in the absorbing reagent.

Procedure for gaseous sampling

8 hour sampling:

Place 30 ml of Tetra-Chloro-Mercurate (TCM) absorbing solution in the standard impinger. Connect the sampling tube leading for manifold of High Volume Sampler. Check the flow rate from rotameter; maintain the flow rate to accurately 1 LPM throughout the sampling period. Shield the absorbing reagent from the direct sunlight during the sampling and after sampling. During hot weather sampling is to be conducted by keeping the impingers impregnated in ice cubes.

24 hourly sampling

Place 50 ml of (TCM) solution in a large impinger and collect the sample at 1 LPM. Determine the air volume by multiplying the airflow rate by the time in minutes. The solution after the sample collection are relatively stable. At the temperature of 250C and above, the losses of SO2 occurs. Therefore, it is advisable to store the samples at 50 C till the analysis.

Analysis of samplesAfter receiving the sample in the lab. check the volume of absorbing media and record it. Normally the volume of absorbing reagent is likely to be reduced as a result of evaporation losses. Make up the evaporation loss by adding fresh, boiled cooled distill water.

Pipette 10 ml of aliquot from the sample into a 25 ml volumetric flask. Prepare a blank solution by measuring 10 ml of unexposed Tetra-Chloro-Mercurate (TCM) solution into 25 ml volumetric flask. Then add 1 ml sulphamic acid and allow to stand for 10 minutes for reaction, then ad 2 ml of formaldehyde and 2 ml of working parasaniline solution. Mix up thoroughly and make up it with freshly boiled and cooled distilled water to the volume. Take absorbance of the



sample after 30 minutes at 560 nm on a spectrophotometer after setting the spectrophotometer at 0.00 absorbance with blank.

CalculationI) The concentration of sulphur dioxide in microgram per meter cube in the sample may be calculated as

follows: (A-Ao) x F x Vf SO2 (/m3) = ----------------------------- Va x Vt

Where

A= Sample Absorbance

Ao = Reagent blank absorbance

F = Calibration factor (g / absorbance unit)

Vf = Final volume of Sample (ml)

Va = Volume of air sampled (cubic meter)

Vt = Volume of sample taken for analysis

II) Conservation of microgram/m3 sulphur dioxide to parts per million (PPM) may be calculated as follows:

SO2 ppm = g SO2/3 x 3.82 x 10-4



Ammonia (as NH3)

Principle: Ammonia is collected in 0.1 N Sulphuric Acid Solution (H2SO4) in a midget impinger to form ammonium sulphate. The solution reacted with nessler reagent to produce a yellow brown complex & determine by colorimetric method at the wavelength 440 nm.

Procedure:

Sampling: Take 20 ml of absorbing solution in midget impinger. Attach the impinger to air sampling pump & draw air through impinger at a rate of 1 lpm for 1hr to 24 hrs. Record the volume of air sample.

Analysis: Take the sample in 50 ml volumetric flask containing 2 ml of alkaline tartrate and makeup to the mark with distilled water. Add 2 ml of nessler reagent to the flask & determine absorbance after 10 minutes at 440 nm in a spectrophotometer. Treat the blank in the same manner as the sample.

Calculation:

Ammonia, g/m3 = Abs ́ F ́ 10 6 V

F- Factor

V- Volume of air sampled, liter

106 – Conversion from liter to cubic meter

Carbonmonoxide (as CO)

SAMPLING: Take the gaseous sample into a bladder through a suction pump.

ANALYSIS: Analyze it on the Gas Chromatograph.

CALCULATION:

Concentration of CO (ppm) = Sample Area x conc.of CO2 in Standard x vol. of standard

Standard Area x vol. of sample



Ozone in Ambient Air (O3)

Principle: Micro amounts of ozone and other oxidant librated iodine when absorbed in a 1% solution of potassium iodide buffered at pH 6.8 ± 0.2. The iodine is determined spectrophotometrically by measuring the absorption of triiodide ion at 352 nm.

Range and Sensitivity: This method covers the manual determination of oxidant concentration between 0.01 to 10 ppm (0.019-19.6mg/m3) as Ozone.

Reagent:

1. Double Distilled Water2. Absorbing Solution: (1% KI in 0.1 M Phosphate Buffer). Dissolve 13.6 gm of potassium dihydrogen phosphate

(KH2PO4), 14.2 gm of disodium hydrogen phosphate (NaHPO4) or 35.8 gm of the dodecahydrate salt (NaHPO4.12H2O) and 10 gm of potassium iodide in sequence and dilute the mixture to 1 lt with double distilled water.

3. Stock Solution: (0.025M) I2 Dissolve 16gm potassium iodide and 3.173gm of resublimed iodine successively and dilute the mixture to exactly 500ml with DDW.

4. 0.001M I2 Solution: Take 4ml of the 0.025 M stock solution into a 100ml low volumetric flask and dilute to the mark with absorbing solution.

Procedure:Take 10ml of the absorbing solution to a midget impinger. Sample at 0.5 to 3 l/m for up to 30 minutes. Calculate the total volume of the air sample, also measure the air temperature and pressure. Do not expose the absorbing reagent to direct sunlight.

Analysis: If appreciable evaporation of the absorbing solution occurs during sampling, add double distilled water to bring the liquid volume to 10ml.

Within the 30 to 60 minutes after sample collection, read the absorbance in a cuvette at 352 nm against a reference cuvette containing DDW.

Measure the absorbance of the unexposed reagent and subtract the value from the absorbance of the sample.

Calculation: The concentration of O3 (ppm) = Total µl ozone per 10 ml Volume of air sample in liter

Lead in Ambient Air (as Pb)

Principle of the Method: Airborne dust samples are collected on cellulose membrane filters (EPM 2000). The filters samples are ashed using nitric acid to destroy the organic matrix and solubilize the lead. The lead content of the ashed material is determined by atomic absorption spectroscopy.

Range and Sensitivity: By atomic absorption the detection limit for lead in aqueous solution about 0.1 g/ml. assuming the ashed sample is diluted to 10 ml this would correspond to 1 g of lead/filter. The optimum working range for Pb extends up to about 10 g/ml.



Reagents:

1. Purity. ACS reagent grade chemicals or equivalent shall be used in all tests. References to water shall be understood to mean double distilled water or equivalent.

2. Care in selection of reagents and in following listed precautions is essential if low blank values are to be obtained.

3. Conc. Nitric acid (68 to 71%) redistilled specific gravity 1.42.

Nickel in Ambient Air (as Ni)

Principle of the Method: Samples are collected by drawing a known volume of air through a membrane or glass fiber filter. The filter samples are ashed, extracted with acid, and the analysis is subsequently made by atomic absorption spectroscopy using 23.9 nm nickel line.

Range and Sensitivity: This method is applicable to the determination of nickel in quantities of 0.1 to 20 g of nickel/ml of solution.

Reagents:

1. Purity. ACS reagent grade chemicals or equivalent shall be used in all tests. References to water shall be understood to mean double distilled water or equivalent.

2. Care in selection of reagents and in following listed precautions is essential if low blank values are to be obtained.

3. Conc. Hydrochloric Acid (36.5 – 38.0%).4. Conc. Nitric Acid (69.0-71.0%).5. Nickel Shot.6. Perchloric acid 72%.7. Hydrochloric acid 1:10. Dilute 100 ml of conc acid to one liter with water.8. Perchloric-Nitric acid Mixture. Add 10 ml of conc perchloric to 90 ml of conc nitric.9.

Benzo[a]Pyrene (BaP) in Ambient Air

Principle of the Method: This rapid method, for the measurement of Benzo[a]Pyrene (BaP) in air samples, is based on the chromatographic separation of air samples extracts on and activated alumina column using a polar solvent, toluene, as the eluting agent. The concentration of hydrocarbon in the eluates is determined from fluorescence emission measurements made on the eluates.

Range and Sensitivity: The method can measure concentrations in a prepared air sample extract or fraction over the range of 0 to 0.25 micrograms of BaP of solution.

Reagents:

1. Cyclohexane. Spectrograde Cyclohexane.



2. Activated carbon.3. Alumina. 100 to 200 mesh size, is heated for 24 hrs in an oven at 1400C before use.4. Toluene. 5. Benzo[a]Pyrene(BaP).6. Standard solutions of BaP. Solutions of BaP are prepared containing 0.005, 0.010, 0.015, 0.020 and 0.025

g/1ml in fluorescence-free toluene. Weigh accurately 1.25 mg of BaP on a micro balance and dissolve in 250 ml of Spectrograde toluene. Measure accurately 1.0 ml of this stock solution and dilute to 1000 ml with Spectrograde toluene. Repeat this with 2.0, 3.0, 4.0 and 5.0 ml portions of stock solution, diluted in each case to 1000 ml.

Procedure: The chromatographic columns are setup in a fume hood and complete preparation of column and elution procedure is carried out there. Fluorescence readings are made while the elutions are in progress.

Using a clean metal punch of cork borer, 4 corcles of 35.5 mm diameter are cut from the high volume glass fiber sample. These represent 1/10.5 of the total effective area of the filter. These are placed in a microsoxhlet extractor on top of a wad of glass wool which prevents the carbon particles from being washed over into the extract and avoids subsequent filtration. The area chose, in this case, amounts to ca 10% of the filter. After 6 to 8 hr extraction with fluorescence-free cyclohexane, the solvent extract is evaporated carefully in a current of nitrogen to 2 ml.

A chromatographic column is then prepared by slurrying the activated alumina with toluene and filling the tube to a depth of 12.0 cm. the concentrated extract is placed on the alumina and after rinsing with a further 1 ml of toluene, elution os carried out using toluene from beginning to end. The first 25 ml of eluate are discarded and 3 ml fractions are collected thereafter up to a total of about 30 fractions. Each fraction is scanned separately in the fluorimeter and those fractions containing BaP and BkF are combined for further measurement.

Having combined all the fractions containing BaP and BkF, these are carefully evaporated and made up to a final volume of 5.0 mol in toluene. Fluorescence emission measurements of peak heights are now made using excitation wavelength 307 and 384 nm.

A blank determination is carried out on the glass fiber filter, glassware and reagents.

Calibration and Standards: Standards curves of fluorescence emission, in arbitrary units, are prepared for the various concentrations of both BaP and BkF at the two exciting wavelengths 384 and 307 nm. i.e., the optimum excitation wavelengths for BaP and BkF. These are prepared by plotting the height of the peaks against the concentration. The fluorescence emission intensities of air sample extracts or fractions are also measured using the same two exciting wavelengths.

Similar calibration curves are obtained when standard solutions are made up in eyelohexane. The sensitivity is noticeable less in toluene than in cyclohexane solution. The emission of BaP with 384 excitation, is higher than the emission of BkF with 384 excitation, so that the toluene based BaP measurement is somewhat better than a measurement made in cyclohexane.

Calculation:

Since the fluorescence emission intensity of BkF is much greater than that of BaP when a mixture of the two is excited at 307 nm, the reading at this wavelength is essentially due to BkF. Having determined the concentration of BkF, one



can calculate the effect of this hydrocarbon when a mixture is excited at 384 nm after which the BaP concentration may be calculated. Thus:-



The concentration of BkF (g/ml) = Emission of Sample at 307 nm excitation Slope of BkF standard curve at 307 nm excitation

The concentration of BaP (g/ml) =

Emission of Sample at 384 nm – (conc. BkF X Slope BkF standard curve at 384 nm excitation)

Slope of BaP standard curve at 384 nm excitation



METHODOLOGY OF SOIL

ANALYSIS



METHODOLOGY FOR PHYSICO-CHEMICAL ANALYSIS OF SOIL

pH

Soils may be acidic, neutral or alkaline in reaction. The pH of soils is significant in crop production and soil management practices because the various degrees of soil reaction are produced by the chemical conditions which exist in soils. pH of soils affects plant growth due to either a depressed solubility of some elements or to an increased solubility of others. It is useful in diagnosing the feasibility of soil. The pH can be taken as negative logarithm of hydrogen ion activity. pH values from 0 to 7 are diminishingly acidic, 7 to 14 are increasingly alkaline and 7 is neutral.

The pH of the soil generally varies from 4 to 8. In humid regions, it is usual to find a soil with

a pH of more than 7.5 or 8 but in arid regions where soluble salts of sodium carbonate accumulate a pH of 9.5 to 11 is sometimes attained. Usually pH of agricultural soils in the humid regions varies from 5 to 6.8. It is also possible to find mineral soils whose pH is 4. Soils having pH < 8.3 are termed alkaline soils.

The determination of pH by conventional chemical means is not practicable and the equilibrium which are involved depend to some extent on temperature. The precise accepted scale of pH can be used only if approximate pH values are required.

The pH determination is usually done by electrometric method which is the most accurate method and free of interference.

ELECTROMETRIC METHOD:

The pH is determined by measurement of the electromotive force of a cell comprising an indicator electrode (an electrode responsive to hydrogen ions such as glass electrode (immersed in the test solution) and a reference electrode (usually a mercury calomel electrode) contact between the test solution and the reference electrode is usually achieved by means of a liquid junction, which forms a part of the reference electrode. The EMF of this cell is measured with pH meter. This is a high impedance electrometer calibrated in terms of pH.

Apparatus:

Glass Electrode:

This must be compatible with the pH meter used and must be suitable for the particular application. Special electrodes are available for pH values greater than 10 and for use at temperature greater than 600 C. Combined glass/reference electrodes are also available and are convenient to use.

Reference Electrode:

The mercury /calomel electrode is widely used but the silver/silver chloride electrode may be preferably used on account of it being more reproducible and more reliable. Les-s .concentrated solutions of KCI (e.g. 3.5 M KCI or 350 gm/litre) are more satisfactory as filling solutions than the saturated solution often used because problems due to clogging of the electrode or the liquid junction will be avoided. To prevent dissolution of the silver chloride film, the potassium chloride filling solution of Ag/AgCI electrodes should be saturated with AgCI.

pH Meter:



Both mains and battery operated models are available; the later type can be used for field’s measurements. The most accurate pH meters can be read to better than = 0.005 pH unit.

Reagents:

1. Buffer solution for pH 4.0

2. Buffer solution of pH 6.8

3. Buffer solution of pH 9.2

NOTE:

In general analytical reagent grade chemicals are satisfactory for the preparation of these solutions. Commercial buffer tablets are available in the market for the preparation of

solution of above pH values (each tablet dissolved in 100 ml gives the buffer solution of required pH),

Procedure:

1. Standardize the pH meter according to the manufacturer's instructions.

2. Select a standard buffer solution with a pH value close to that of the soil to be tested.

3. Set the temperature control to the temperature of the buffer.

4. Set the meter to the pH of the buffer at that temperature.

5. Check the electrode response by measuring a second standard buffer solution of different pH.

6. Wash the electrode thoroughly first with distilled water and then with the sample.

7. Set the temperature control to the temperature of the sample.

8. Add 100 ml distilled water to 40 g soil.

9. Stir the mixture for 10 minutes, allow to stand for 30 minute, stir again for 2 minutes.

10. Measure the pH of the soil suspension.

11. Immerse electrodes in the sample and record the pH after stabilising the system.

Note:

Between measurements, the electrodes are kept in distilled water. New or dried out glass electrodes should be prepared for the use by soaking in 0.1 N HCI for 8hours or according to the manufacturer's instructions.



CONDUCTIVITY

Conductivity is a capacity of water to carry an electrical current and varies both with the number and types of ions the solution contains, which in turn is related to the concentration I of ionized substances in the water. Most dissolved inorganic substances in water are in the ionized form and hence contribute to conductance. The electro- conductivity measurement identifies soils which are potentially saline. The electro- conductivity of saturated paste I extract is measured to determine the level of salinity.

Conductivity measurement is affected by:

1. The nature of the various ions, their relative concentration and the ionic strength of water.

2. Dissolve CO2

3. Temperature (for precise work, the conductivity must be determined at 250 C.

Instruments:

Most of the instruments commercially available for measurement of conductivity consist of.

1. A source of alternating current.

2. A wheat-stone bridge, a null indicator, and,

3. A conductivity cell consisting of a pair of rigidly mounted electrodes, each conductivity cell has its own cell constant: depending on its shape, size and the position of the electrodes. Either the cell constant is mentioned by the supplier or can be determined by using standard solution of KCl (0.01 M). Alternatively, by comparison with a cell of known cell constant. Other instruments measure the ratio of I ~ alternating current through the cell to voltage across it and have advantage of linear reading of conductance. Portable battery operated instruments for both pH and conductivity are also available for field studies.

Conductivity can be measured as per the instruction manual supplied with the instrument and the results may be expressed as siemens I metre or 11 siemens I cm at temperature say 250 C at which measurement was made. With reasonable care I conductivity meter needs very little maintenance and gives accurate results. However few important points in this respect are:

1. Adherent coating formation of the sample substances on the electrodes should be -avoided which requires thorough washing of cell with distilled water at the end of each measurement.

2. Keep the electrode immersed in distilled water.

3. Organic material coating can be removed with alcohol or acetone followed by washing with distilled water.



Reagents:

1. Dissolve 0.7456 g of KGl in 1000 ml of distilled water. It is equivalent to 1.412 mhos/cm conductivity at 250 G.

2. Dissolve 7.456 g of KGI in 1000 ml of distilled water. It is equivalent to 12890 Jlmhos/cm.

Procedure:

1. Add 100 ml distilled water to 40 g soil.

2. Stir the mixture for 10 minutes, allow to stand for 30 minutes, stir again for 2 minute.

3. Allow to settle for 1 hour then measure the conductivity of the supernatant liquid.

Calculation = Observed conductance x Cell constant x temperature factor at 250 C.

Temperature Factor Temperature Factor

3 1.62 18 1.14

4 1.58 19 1.12

5 1.54 20 1.10

6 1.50 21 1.08

7 1.46 22 1.06

8 1.42 23 1.04

9 1.39 24 1.02

10 1.36 25 1.00

11 1.33 26 0.98

12 1.30 27 0.97

13 1.27 28 0.95

14 1.24 29 0.93

15 1.21 30 0.92

16 1.19 31 0.90

17 1.16 32 0.89

BULK DENSITY

Bulk density of the soil is the dry weight of a unit volume of it. It is expressed as g/cm3. Generally, the bulk density has been found in the range of 1.1 to 1.5 g/cm3 for medium to fine textured soil and from 1.2 to 1.65 g/cm3 for coarse



textured soil. However, it has been slightly higher in case of alkaline soils. The soils having high bulk density have been found to be inhibitive to root penetration and have low permeability and infiltration. The bulk density is inversely related to pore space of soil.

Apparatus Oven, Measuring Cylinder and Chemical Balance.

Method Collect the sample the dry it in an over at 1050 C until constant weight. Now put a little dried soil in a measuring cylinder and record the volume. Now find out the weight of this volume of soil in a chemical balance.

Calculations:

Bulk Density = Weight of dry soil (g) = g/cm3 Volume of dry soil g/cm3

Bulk Density = W2 -W1 = g/cm3 V

W1 = Weight of empty watch glass in gm.

W2 = Weight of empty watch glass and soil in gm.

V = Volume of soil in cm3

WATER HOLDING CAPACITY

When soil is soaked with water, water fills all the pores between the par1icles of soil and no air space exists as in the case of aquatic sediments. Such a soil is said to be at its maximum water holding capacity or saturation.

Apparatus :-

Perforated Circular Soil boxes, Filter Paper Whatmann No. 1, Petri Dish, Oven and Chemical Balance

Method

Collect the soil sample and crush it. Dry this sample in an oven at 105 0C. Keep a filter paper (Whatmann No.1) inside the perforated bottom of the circular soil box. Then weigh the box. Now fill it with dried soil sample. Then, find out the weight of the box filled with dried

soil. Keep the box in petri dish of 10 cm diameter having water for about 12 hours, so that water enters the box and gets saturated the soil. Remove the box out of water from petridish, wipe it dry on the outside and find out its weight.

Calculations

Water Holding Capacity = (W3 -W2) - (W2 -W1) W2 -W1

Where W1 = Weight of empty box

W2 = Weight of box filled with dried soil

W3 = Weight of box with water saturated soil.



SOIL PARTICLE SIZE ANALYSIS

Principle

The particle size analysis of soil estimates the percentage sand, silt and clay contents of the soil and is often reported as percentage by weight of oven-dry and organic matter-free soil.

The analysis is usually performed on air-dry soil. Based on the proportions of different particle sizes, a soil textural category may be assigned to the sample.

The first stage in a particle size analysis is the dispersion of the soil into the individual particles. These are the sand (2.00 -0.5 mm), silt (0.05 -0.002 mm) and clay «0.002 mm) fractions. Individual soil particles are often bound into aggregates hence the requirement for dispersion.

The hydrometer method of silt and clay measurement relies in the effects of particle size on the differential settling velocities within a water column. The setting velocity is also a function of liquid temperature, viscosity and specific gravity of the falling particles. Theoretically the particles are assumed to be spherical and to have a specific gravity of 2.65. If all other factors are constant then the settling velocity is proportional to the square of the radius of the particle (Stoke's law). In practice, therefore, correction for the for the temperature of the liquid is made. Greater temperatures result in reduced viscosity due to, liquid expansion and a more rapid descent of falling particles.

Reagents and equipment

Calgon (sodium hexametaphosphate) solution 10%. Dissolve 100 gm of calgon in 1 litre of distilled water. This solution should not be kept over one month, when too o1d it loses its dispersing efficiency because if will be converted to another compound.

Amyl Alcohol

Hydrometer with Bouyoucos scale in gm litre.

Soil dispersing stirrer. A high speed electric stirrer with a cup receptacle.

Procedure

1. Weigh out 50 9 of air -dry <2 mm soil (100 gm in case of very sandy soil) into a 400 ml beaker.

2. Saturate the soil with distilled water and add 10 ml of 10% Calgon solution. Allow to stand for 10 minutes.

3. Transfer the suspension to the dispersing cup and make to the mark in the cup with distilled water.

4. Mix the suspension of 2 minutes with an electric high speed stirrer. Use ordinary bottles if a cup is not available. Shake the suspension overnight if no stirrer is available.

5. Transfer the suspension into a graduated cylinder and rinse remaining soil into the cylinder with distilled water. Insert the hydrometer into the suspension and add water to 1130 ml, then remove the hydrometer.



6. Cover the cylinder with a tight fitting rubber bung and mix the suspension by inverting the cylinder carefully ten (10) times. Note the time.

7. Quickly add 2-3 drops of amyl alcohol to the soil suspension in order to remove froth and after 20 seconds place the hydrometer gently into the column.

8. At 40 seconds take the hydrometer reading and measure the temperature of the suspension.

9. Repeat step 6 (mixing of the soil suspension 10 times) and allow the cylinder to stand undisturbed for 2 hours.

10. After two hours take both hydrometer and temperature readings.

11. Make the necessary temperature corrections (Table 1). Temperature affects the hydrometer readings and, because the hydrometer has been calibrated at 680 F (200 C), either correction factors must be applied or the determination conducted in a temperature controlled room kept at the correct temperature.

Calculations

Percent Sand: After 40 seconds, the sand present in 1 liter of the suspension, subtract this value from the original sample weight. For example, if the hydrometer reading after 40 seconds corrected for temperature is 18.0 g/liter, then silt + clay weight 18.0 g in the 1 liter soil suspension. Therefore, the sand weights 50.0 -18.0 = 32.0 g in the 1 liter suspension (of the original 50.0 gm air-dry soil sample). The percentage sand is calculated by dividing the sand content (32 g) by the total (50 g) and multiplying by 100 as follows:

Sand % = 32.0 x 100 = 64%

50.0

Percent Clay: After 2 hours, the silt has settled. The hydrometer reading now reflects the -clay content of the original suspension. For example, if hydrometer reading after temperature correction is 4.7 g/litter, then the percentage of clay in soil is

Clay % = 4.7 x 100 = 9.45 50.0

Percent Silt: The silt content is calculated by subtracting the sum of the clay and sand contents from 100% or:

Silt % = 100 - (9.4% clay + 64% sand) = 26.6%

Soil Texture: Once the sand, silt and clay distribution is measured, the soil may be assigned to a texture class based on the soil textural triangle (Figure 1). Within the textural triangle are various soil textures which depend on the relative proportions of soil particles. Users simply obtain the appropriate texture based on the particle size distribution. In the example, above (64% sand, 27% silt and 9% clay), the corresponding soil texture is a sandy loam.

Table 1: Temperature correction for hydrometer readings of soil texture.

Temperature (0C) Hydrometer correction g/liter

15 - 2.016 - 1.517 - 1.018 - 1.0



19 - 0.520 Nil21 + 0.522 + 0.523 + 0.524 + 0.525 + 0.5

Procedural notes

1. Cylinders for particle size analysis are calibrated depending upon the volume of the hydrometer in use.

AVAILABLE NITROGEN

Principle:

Nitrogen is a major element essential for plant growth and it is a constituent of all proteins and nucleic acids, It is generally taken up by plants as ammonium (NH4) and nitrates (NO3) ions, The ammonium ions and nitrates ions are jointly make up to available nitrogen in soil, The two major forms of available nitrogen, ammonium and nitrate produces a more rapid and spectacular effect on the growth of plants than any other nutrients, This reflects the need to measure the herds and subsequent movement patterns of these ions in soils during cropping in order to give firm recommendations on fertilizer N/manure/crop residue uses,

Because of rapid transformations of N to various forms, many procedures have been developed to measures these have two ions (NH4 + NO3) in soils, These include the biological and chemical methods, It has been demonstrated that the chemical methods is suitable for predicting the natural available soil over a wide range of soils, The method gives measurements of NH4 N and NO3 N in a single soil extract.

Extraction Procedure:

Weigh 10 gm freshly sampled soil (or soil kept in the refrigerator) into a plastic shaking bottle. Add 100 ml of 2 N KCl extracting solution. Stopper and shake contents for 1 hour.

Filter through whatman no. 42 filter paper if analysis will not be completed in one day, store the filtrate in the refrigerator. Microbial activity associated with N mineralization may also be suppressed by storing the extract in a refrigerator when the distillation cannot be conducted immediately.

Ammonia Distillation

1. Set up the ammonia distillation apparatus.

2. Pass steam through the apparatus for 30 min. Check the steam blank by collecting 50 ml distillate and titrating with 0.002 N H2SO4. The steam blank should not require more than 0.2 ml of acid.

3. Check also the 2 M KCI for possible contamination by steam distilling 10 ml of this solution.

4. Add 25 ml of boric acid indicator solution to a 250 ml conical flask.

5. Place the flask under the condensor of the steam distillation apparatus so that the tip of



the condensor is within the surface of the boric acid indicator solution.

6. Pipette an aliquot of 10 ml of the soil extract into the distillation flask and add sodium

hydroxide solution directly to the bulk of the distillation flask. Start distillation by closing the stop cock on the steam by pass tube.

7. When the distillate is collected about 50 ml in the conical flask. Stop the distillation by opening the stop cock removing the burner. Rinse the tip of the condensor with a little distilled water.

8. Determine the ammonia nitrogen content in the distillate by titration with 0.002 N H 2SO4 .the colour change at the end point is from green to a permanent faint pink. At the end point 1 ml of 0.002 N H2SO4 = 28 I.1g NH3 N2.

Calculation

Since 100 ml KGI is used to extract NH4 – N and NO3 -N from 10 g soil, then 10 ml KCl

(aliquot in distillation) is used to extract:

10 x 10g Soil = 1 gm of soil 100 from titration 1 ml of 0.002 N H2SO4 = 28 I.1g NH3 -N

Therefore quantity of NH4 -N in 1 gm soil = ml of 0.002 N H2SO4 x 28 g

for data correction on soil dry (1030 G) basis. The procedure is as follows:

W1 = Weight of empty crucible.

W2 = Weight of empty crucible + fresh soil

W3 = Weight of empty crucible + dry soil

W3 - W1 W2 - W1 Hence the quantity of NH4 -N in 1 gm of oven dry.

Soil = ml of 0.002 N H2SO4 = 28 X (W3 -W1)/(W2 -W1) g

AVAILABLE PHOSPHORUS

Principle

The availability of soil phosphorus to plants varies greatly depending on reaction, mineralogical composition, type of colloids present and content of organic matter in the soil. In many instances. phosphorus occurs in the soil in the form of ion and aluminium phosphorus. These compounds are only slowly or partially available to plants. The fluoride ion has the special property of complexing aluminium and ferric ions in acid solution with consequent release of phosphorus held in the soil by these trivalent ions. The dilute acid fluoride procedure is extensively used for the extraction of



available phosphorus of soils with -0.03 N NH4 F and 0.05 N HCI and has been found to give results that are highly correlated with crop response to phosphate fertilization.

Reagents:

Ammonium fluoride. NH4 F. 1 N: Dissolve 37 g of AR NH4 F in distilled water and dilute the

solution to one litre. Store the solution in a polythene bottle.

Hydorchloric acid. HC/. 0.5 N: Dilute 44.2 ml of AR conc. HCI (11.2 N approx.) to 1000 ml with distilled water

Soil extracting solution. or Bray p2 solution: Add 150 ml of 1 N NH4 F solution and 1000 ml of 0.5 N HCI to 3850 ml of distilled water placed in a 5 litre container. This gives a solution which a 0.03 N NH4 F and 0.1 N HCI. It keeps in glass more than one year.

Boric acid. H3BO3. 0.8 M: Weight out 49.4 g of AR H3 B03 powder (AR) into 1 litre volumetric flask Dissolve and dilute to mark with distilled water.

Ammonium molybdate antimony potassium tartrate solution (mixed reagent): Dissolve 6 g -ammonium molybdate (AR) in 125 ml of warm (50 0C) distilled water. Dissolve 0.1455 g of 'wi antimony potassium tartrate in 50 ml of distilled water. Add both solutions to 500 ml of 5 N

H2SO4 which has been transferred to a 1 litre volumetric flask. Mix thoroughly and dilute with distilled water to 1 liter. Transfer to a brown reagent bottle. Store in a dark, cool place. The mixture keeps for 2 months.

Ascorbic acid reducing agent: Dissolve 1.054 g ascorbic acid in 200 ml of ammonium required on the day of analysis. The solution keeps of about 24 hours.

Phosphate standard stock solution: Weigh accurately 1.0982 g of dry KH2P04 (AR).

Transfer to a one litre volumetric flask. Dissolve in distilled water and make up to volume (1000 ml). The concentration of P is 250 mg/P/1000 ml, or 0.250 mg/P/ml.

Procedure:

1. Soil extraction: Weight accurately 2.5 g of dry soil (2 mm) into a 250 ml plastic bottle. Add 50 ml of Bray P-2 extracting solution and shake for 5 minutes. Filter through Whatmann NO. 42 filter paper. If filter is not clear, pour the solution back through the filter.

2. Pipette 10 ml of each phosphorus standard solution and 10 ml of soil extract into 50 ml volumetric flasks.

3. Add about 20 ml of distilled water to each flask.

4. Add 5 ml of 0.8 M boric acid solution to each flask.

5. Add 10 ml of ascorbic acid solution to each flask.

6. Make to the mark with distilled water.

7. Stopper and shake contents well.

8. Measure the intensity of blue color at 880 nm after 10 minutes and before 30 minutes. Preparation of Calibration curve: Pipette 1, 2, 5, 10, 15 and 20 ml of phosphate standard solution into a 100 ml volumetric flask. Add 10 ml of soil extracting solution, 10 ml of ascorbic acid reagent to each flask and fill upto the mark. After at least 10 minute



but not more than 30 minute, measure the absorbance of each sample at 880 nm using reagent blank as the reference solution. Plot absorbance Vs phosphate concentration to give a straight line passing, through the origin. Test at least one phosphate standard with each set of samples.

Calculations:

mg/P/100 gm of soil = Phosphate reading in mg from the graph x 100 gm of soil. 0.5



CALCIUM CARBONATE

Introduction:

Inorganic carbonates either accumulates in the soil by pedogenic processes or inherited from calcareous parent materials. It is used to define carbonatic, particle size, calcareous soil classes, calcic and petrocalcic soil horizons. Its presence may lead to some nutrient deficiencies in the soil. Methods of quantitative determination of calcium carbonate includes dissolution of carbonates in acid and determination of carbon dioxide by titrimetry and by measuring the volume of evolved carbon dioxide.

Principle

The dried soil sample 2 mm is reacted with hydrochloric acid and evolved carbon dioxide gas is absorbed in dilute hydrochloric acid and the remaining hydrochloric acid is titrated with sodium hydroxide.

Reagents & Apparatus: Chemical Balance

i) Standard 1N HCI. Dilute 88 ml of concentrated HCI to 1000 ml standardize it against standard NaOH.

ii) Standard in NaOH. Solution 1 N; Dissolve 40 gm NaOH to 1000 ml of distilled water and standardize using methyl red indicator.

iii) Phenolphthalein Indicator: Dissolve 0.5 g of phenolphthalein in 50 ml 95% ethyl alcohol and 50 ml of distilled water.

Procedure:

Weigh 5 g of dry soil accurately and transfer to 250 ml beaker and add 100 ml of 1 N HCI solution. Cover with a watch glass and stir several times for one hour at interval of 10 minutes. After settling for 10 minutes, pipette off 20 ml of supernatant liquid and take into a conical flask. Add 6 to 8 drops of phenolphthalein indicator and titrate with 1 N sodium hydroxide solution till the solution turns pink.



Calculations:

1 ml of 1N HCI is equivalent to 0.05 gm of CaCO3 present in the soil sample.

Carbonate present in soil percent =

Volume of hydrochloric acid consumed for 5 gm of soil x 0.05 x 100 5

ORGANIC CARBON

Principle

Organic carbon present in the soil is determined by digestion with excess of potassium dichromate and sulphuric acid and the unutilized potassium dichromate is then titrated with ferrous ammonium sulphate using diphenylamine as indicator. The used potassium dichromate the difference between added and residual potassium dichromate gives a, measure of organic carbon content of soil.

The elementary carbon present as graphite, charcoal etc. is not attacked in this method. The recovery of the carbon in this method is not 100 percent. Only about 60-90 percent of the total organic carbon is recovered depending upon the kind. For example in most cases, the proteins remain unaffected by this method.

Reagents

1. Potassium Dichromate Solution 1 N. Dissolve 49.04 gm of K2Cr2O7 in distilled water and dilute to 1000 ml. 2. Sulphuric Acid concentrated H2SO4 (Sp gravity 1.84) 3. Phosphoric Acid H3PO4 concentrated (Sp gravity 1.71).4. Ferrous Ammonium Sulphate 0.4 N. 5. Dissolve 156.86 g Fe (NH4)2 (SO4)3 6H2O in distilled water and add 14 ml conc. H2SO4 and dilute to 1000 mi. 6. Diphenylamine Indicator 7. Dissolve 0.5 diphenylamine in a mixture of 20 ml distilled water and 100 ml conc. sulphuric acid. 8. Sodium Fluoride

Procedure

1. Take oven dried soil sample and pass through 0.2 mm non ferrous screen. 2. Weigh a suitable quantity of soil not exceeding 10 gm (containing about 10-25 mg carbon) and transfer to a

dried 500 ml conical flask. 3. Add 10 ml 1 N K2Cr2O7 solution and 20 ml conc. H2SO4 and mix by gentle swirling. 4. Keep the flask to react the mixture for about 30 minutes. 5. After the reaction is over, dilute the contents with 200 ml of distilled water and add 10 ml of phosphoric acid

and 0.2 gm sodium fluoride followed by 1 ml of diphenylamine indicator. 6. Titrate the sample with 0.4 N ferrous ammonium sulphate till the dull green color changes to brilliant green. 7. Run a blank with same quantity of chemical but without soil. 8. If more than 8 ml of the 10 ml added K2Cr2O7 is consumed (ml titrant less than 5 ml), repeat with less quantity

of the sample.



Calculation

Percent Carbon = 3.939 1 - T g S

g = weight of soil sample in gms.

S = ml ferrous ammonium sulphate solution with blank titration.

T = ml of ferrous ammonium sulphate solution with sample titration.

% Organic matter = % C x 1.724


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